CN104291301B - A kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer - Google Patents
A kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer Download PDFInfo
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Abstract
The present invention relates to chemical technology field, especially a kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer, it is changed by the coefficients such as the temperature of dikalium phosphate being prepared by phosphoric acid by wet process, improve the purity of dikalium phosphate product, the Chemical Mixed Fertilizer containing N, P, K chemical combination state can be produced simultaneously, and in filtrate, add a kind of controlled-releasing compounding fertilizer of formaldehyde making.The method is possible not only to improve the purity of dikalium phosphate, the absorbance of this osmanthus fragrans special fertilizer produced is good, this osmanthus fragrans special fertilizer simultaneously produced disclosure satisfy that the nutritional need in each period in osmanthus fragrans growth cycle, has greatly facilitated osmanthus fragrans growth, is efficient Chemical Mixed Fertilizer.
Description
Technical field
The present invention relates to chemical technology field, particularly relate to a kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer.
Background technology
Dikalium phosphate, it is widely used in the crop of the almost all types such as all types of industrial crops, grain, melon fruits and vegetables, have notable increasing both production and income, the amount of changing optimizes many excellent effects such as quality, resistant to lodging, disease and insect resistance, preventing and treating senilism, and there is the malnourished effect overcoming the aging absorbability of plant growth later stage root system to decline and to cause, belong to novel high density phosphorus potassium Was Used compound fertilizer, be efficient phosphorus potassium complex fertilizer agriculturally.Current domestic a lot of fertilizer producers are all producing dikalium phosphate compound fertilizer, its production method mainly has neutralisation, extraction, ion exchange, double decomposition, direct method, crystallization process and electrolysis etc., wherein double decomposition includes thermal phosphoric acid and phosphoric acid by wet process produces dikalium phosphate, and thermal phosphoric acid cost is bigger, should not as being widely popularized, therefore, Wet-process Phosphoric Acid Production dikalium phosphate product becomes main method, and the basic step of wet process phosphoric acid for preparing phosphoric acid is as follows:
Reaction equation one:
CO(NH2)2+H3PO4=CO (NH2)2.H3PO4
Reaction equation two
CO(NH2)2.H3PO4+ KOH=KH2PO4+H2O+CO(NH2)2
React at 40～80 DEG C in whole reaction, there is not any change after the completion of reaction in substantial amounts of phosphoamide, simultaneously because phosphoamide dissolubility is significantly high, when 20 DEG C, its dissolubility is 85g/100ml (referring to " phosphate fertilizer and compound fertilizer " the 20th volume the 6th phase solubility of chemical fertilizer and Compound fertilizer production technology), the simultaneously rising of the solubility with temperature of phosphoamide and increase, so the phosphoamide contained in filtrate is after passing through cooling crystal precipitation, possibly together with a large amount of undecomposed phosphoamides, K in filtrate+、H2PO4 -、HPO4 2-、PO4 3-If directly doing waste water and discharge, both having wasted resource, and can cause again the waste of resource, meanwhile, the purity of the dipotassium hydrogen phosphate crystal of precipitation is not high.
Flos Osmanthi Fragrantis (formal name used at school: Osmanthusfragrans), for temperate zone seeds, is the famous flower variety of China, has important ornamental value, be also the important source material of food industry, fragrance industry, light industry.Flos Osmanthi Fragrantis concentrates on and blooms 9～October, generally blooms 2～3 times.Present cultigen, uneven owing to mineral elements content is low, fertilizer efficiency is short, between element, cause Flos Osmanthi Fragrantis florescence undernutrition, nutritional deficiency and the problem such as pattern is of poor quality occur, need imposing fertilizer or spraying Quick-dissolving fertilizer repeatedly in time.Not only increase the amount of labour of flower-grower, and the utilization rate of fertilizer is low, cause that the management of Flos Osmanthi Fragrantis is relatively costly.
According to another report:
Carbamide, carbon ammonium plant absorption utilization rate be: 20% one 46%；
The plant absorption utilization rate of phosphate fertilizer (diammonium, an ammonium, triple superphosphate) is: 10% one 25%；
The plant absorption utilization rate of common potash fertilizer is: 45% one 60%.
Unabsorbed mixing fertilizer, easily cause soil compaction, mixing simultaneously fertile release and lose too fast, early stage can cause the overgrowing of osmanthus fragrans, later stage is due to osmanthus fragrans overgrowing and because rainwater soaks or fertilizer self decomposition, cause the nutrition in soil cannot supply the needs of osmanthus fragrans, cause the growing way of osmanthus fragrans slow down or rest.
For in Wet-process Phosphoric Acid Production dikalium phosphate process, the purity of dikalium phosphate is not high, possibly together with a large amount of undecomposed phosphoamides, K in filtrate+、H2PO4 -、HPO4 2-、PO4 3-Deng material, the researcher of the present invention is from substantial amounts of prior art literature and exploration for many years and research, and the tradition component content of osmanthus fragrans special fertilizer and the absorbing state of osmanthus fragrans are studied, effectively inquire into out from the filtrate of Wet-process Phosphoric Acid Production dikalium phosphate, produce osmanthus fragrans special fertilizer, the purity solving Wet-process Phosphoric Acid Production dikalium phosphate is not high, in filtrate, effective ingredient such as cannot utilize at the problem, the absorbance of this special fertilizer is good simultaneously and the effect of realizing controlled-release, at home in fertilizer production, have no report.
Summary of the invention
For above technical problem, the invention provides a kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer, by unique process production design, improve the purity of dikalium phosphate, make full use of the effective ingredient of wet process phosphoric acid for preparing dikalium phosphate simultaneously, produce out the osmanthus fragrans special fertilizer of applicable osmanthus fragrans growth.
The present invention is achieved by the following technical solutions:
A kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer provided by the invention, mainly comprises the steps that
1) adopting phosphoric acid is (1.2-1.5) with phosphoamide according to mol ratio: 1 mixes, and is warming up to 160 DEG C for 6 DEG C/min from 80 DEG C with programming rate, stirring reaction 4-5h, and separation obtains intermediate；Adopting this intermediate again is 1:(1.1-1.4 with alkaline potassium salt according to mol ratio) mix, adjustment pH value is 8.5-9.0, after reaction terminates, obtain slip nitrogenous, phosphorus, potassium, and the slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer and cools to 35～40 DEG C, carry out crystallization filtration treatment, make filtrate circulation crystallization in cooler crystallizer process, the filter cake obtained is dikalium phosphate product, the component content in detection filtrate；
2) in filtrate, formalin is added, it is (0.8～0.9) according to the mol ratio with the phosphoamide contained in solution: 1 mixes, with calcium hydroxide, potassium hydroxide and phosphoric acid solution regulate the pH value of solution, when the pH value detected in solution is 18-25% at the content of 8.5～9.0 nitrogen components, phosphorus composition content is 4-8%, when potassium component content is 12-16%, when calcium component content is 12～18%, mixed liquor is put in retort, pressure is increased to 8～10 atmospheric pressure, be rapidly heated 85 DEG C time, ramp with 5～6 DEG C/min, when reaching 120 DEG C, keep 2～3h；
3) by step 2) solution that obtains is divided into two parts,
The solution fast cooling taking a deal to 60 DEG C and is depressurized under normal pressure and stands, called after solution A,
The solution taking a deal is put in a retort, when atmospheric pressure is quickly ramped up to 2 atmospheric pressure, increases atmospheric pressure with the speed of 50～100Pa/min, simultaneously temperature is from 85 DEG C of ramp with 1～2 DEG C/min, when reaching 3 atmospheric pressure, temperature is when reaching 95 DEG C, keeps 0.5～1h, called after solution B；
4) by step 3) solution A that obtains, it is cooled to 60～65 DEG C after B mixing, and add a certain amount of H2SO4Solution, regulates the scope of pH to 7.0～7.4, adds at least one in a small amount of zinc sulfate, copper sulfate, manganese sulfate, ammonium molybdate, ferrous sulfate, chelated iron, Borax, stands 0.5～1h, obtains solution C；
5) by step 4) in the solution C that obtains be cooled to 20～25 DEG C, carry out crystallization filtration treatment, obtain substantial amounts ofThe potassium phosphate of root, and a small amount ofWithDeng the chemical combination state compound fertilizer just finished product of urea aldehyde；
6) pelletize is dried, in this step, first by step 5) mixture that precipitates out is fabricated to the granule that diameter is 0.2～0.4cm, be subsequently placed in temperature be 45～50 DEG C, flow velocity be 3～4m/s ammonia environment in dry, make osmanthus fragrans special fertilizer.
Further, described calcium hydroxide concentration is 35～40%, and the concentration of described potassium hydroxide solution is 20～25%, and the concentration of described phosphoric acid solution is 20～25%.
Further, described step 4) sulfuric acid concentration be 5～15%.
Further, when the content of the nitrogen component in chemical combination state compound fertilizer just finished product is 16-19%, phosphorus composition content be 3-7%, potassium component content be 11-14% time, calcium component content be 10-15% time, stop crystallization.
Further, described osmanthus fragrans special fertilizer is the Chemical Mixed Fertilizer of chemical combination state.
In the present invention, by carbamide and phosphoric acid at 80 DEG C, and it is warming up to the speed of 5 DEG C/min under the environment of 160 DEG C and reacts, generate urea phosphate, and being stepped up along with temperature, and then make the coordinate bond dialysis between urea phosphate form two kinds of ion like materials, namely it is exactlyWithWhenIon is in phosphoric acid environment, it will close with phosphoric acid, and then carries out ionic polymerization under the temperature environment when urea phosphate coordinate bond dialysis so thatIon generates with phosphoric acidIntermediate-ion, makes containing substantial amounts of dihydrogen phosphate in solution simultaneously, and when adding potassium ion compound, dihydrogen phosphate and potassium ion react generation dikalium phosphate, and in succession reach capacity；When potassium content is excessive, it will react with the ammonium radical ion in intermediate-ion, intermediate-ion chelating is further made to becomeIntermediate-ion, and with positive charge, and then when solution participates in other electronegative ions or compound, it will form compound salt with this ion, the further nutritional labeling in abundant product.
Meanwhile, carbamide, can react with formalin at pH under 8.5～9.0 alkaline case, generatesDeng urea aldehyde series of products,Not easily preserving under alkaline case Deng urea aldehyde series of products, so needing the pH value with sulfuric acid solution adjustment solution when 7.0～7.4, precipitating out the time preserved longer.SimultaneouslyDeng urea aldehyde series of products after fertilising, under the effect of microorganism, the N, the C element that are easily absorbed by plants can be discharged, the chain length of its urea aldehyde is more long, chain needs the time ruptured more long, and the time producing fertilizer efficiency can discharge after a certain time, it is possible to reaches the effect of slow release.
The beneficial effects of the present invention is:
Compared with prior art, there is following characteristics in the present invention:
1. rich in carbon amide solution in the filtrate of conventional wet lay phosphoric acid dikalium phosphate, the dissolubility at the same temperature of phosphoamide is relatively large, and isolated phosphoamide crystal is rich in KH2PO4In other crystal, entered in the filtrate after cooling precipitates out phosphoamide crystal possibly together with substantial amounts of phosphoamide, K simultaneously+、H2PO4 -、HPO4 2-、PO4 3-Utilize Deng not operatively, the temperature of wet process phosphoric acid for preparing dikalium phosphate is regulated to 80～160 DEG C by the present invention, and react from the environment of 80 DEG C to 160 DEG C with the speed intensification of 5 DEG C/min, not only make the dikalium phosphate product purity of precipitation reach more than 98%, filtrate also generatesCation, to filtrate crystallisation precipitate out generate chemical combination state Chemical Mixed Fertilizer go out finished product time, it is ensured that chemical combination state Chemical Mixed Fertilizer goes out in finished productIntermediate-ion and dihydrogen phosphate, and between C and O, form coordinate bond, this intermediate-ion can form multielement intermediate-ion with centering element compound chelating, and then can continue to the compound electronegative with other or ion formation chelate, improve constituent content in double salt, and then the nutrient content in the double salt that this ion exists can be adjusted, simultaneously, this chelate can be hydrolyzed again and by crop, and then effectively long-term can provide fertilizer efficiency for crop, simultaneously, in conjunction with the mensuration of constituent content in the solution that this ion is existed, and then adjust each constituent content when double salt is formed, dry and obtain chemical combination state double salt compound fertilizer, its absorbance is fabulous, reduce osmanthus fragrans planting cost and improve osmanthus fragrans quality；
2. containing phosphoamide composition partly in filtrate, add formalin, under alkali condition and certain pressure intensity and temperature, generateDeng urea aldehyde series compound fertilizer, it is possible to make this osmanthus fragrans special fertilizer reach the effect of realizing controlled-release；
3. in granulating and drying process, pass into the ammonia that flow velocity is certain, it is possible to absorbed nitrogen element further, can quickly be absorbed by plants after fertilising, ensure that the supply of osmanthus fragrans early stage nutrition further；
4. this osmanthus fragrans special fertilizer has the advantages that absorbance is good, realizing controlled-release formula is good.
Detailed description of the invention
Below in conjunction with specific embodiment, the concrete technical scheme of the present invention is described in detail.
Principle illustrates:
The present invention carries out research and discussion by the mechanism that phosphoric acid and phosphoamide are reacted, and recognizes in conjunction with prior art literature, and phosphoric acid and phosphoamide react generation urea phosphate, and its molecular formula is: CO (NH2)2.H3PO4Under the environment of higher temperature, the chemical bond meeting dialysis between H and O in phosphoric acid, hydrion is combined with carbamide and forms the ionic state containing positive charge, urea phosphate is made to form the ion double salt that a kind of positive and negative charge attracts mutually, its mechanism structural response following expression: CO (NH2)2.H3PO4→(H2PO4)-.(H2NCONH3)+
Further, urea phosphate ion double salt under the environment that phosphoric acid exists, (H therein2NCONH3)+Cation is close with phosphoric acid, forms the intermediate-ion of C → O coordinate bond, is (CO5PN2H8)+, and then make in urea phosphate intermediate containing substantial amounts of (H2PO4)-(CO5PN2H8)+Ion, when adding excessive and appropriate potassium ion, dihydrogen phosphate and potassium ion form dikalium phosphate crystal and are precipitated, unnecessary potassium ion and (CO5PN2H8)+Ionic reaction, and displace part NH4 +So that containing (CO in solution5PNH4K)+Double salt ion, and analyze and control the content of N in solution, P, K element by detecting, heat drying can be prepared by containing N, P, K element chemical combination state compound fertilizer.
Its concrete reaction principle will carry out further instruction by following reaction structure formula and reaction mechanism:
Reaction equation one:
CO(NH2)2+H3PO4→CO(NH2)2.H3PO4
Reaction equation two:
Reaction equation three:
Wherein, the dotted line between carbon atom and oxygen atom represents there is coordinate bond between C atom and O atom.
Reaction equation four:
Wherein, the dotted line between carbon atom and oxygen atom represents there is coordinate bond between C atom and O atom.
In the present invention, carbamide and formaldehyde are being under 8.5～9.0 alkaline case at pH value, can produce reaction:
Reaction equation five
Reaction equation six
GenerateDeng urea aldehyde series of products,Not easily preserving under alkaline case Deng urea aldehyde series of products, so needing the pH value with sulfuric acid solution adjustment solution when 7.0～7.4, precipitating out the time preserved longer.SimultaneouslyDeng urea aldehyde series of products after fertilising, under the effect of microorganism, the N, the C element that are easily absorbed by plants can be discharged, the chain length of its urea aldehyde is more long, chain needs the time ruptured more long, and the time producing fertilizer efficiency can discharge after a certain time, it is possible to reaches the effect of slow release.
Noun illustrates:
Urea phosphate (Ureaphosphate, UP), No. CAS is 4861-19-2, and molecular formula is CH7N2O5P, is represented by CO (NH2)2·H3PO4:
It it is a kind of fine chemical product being widely used in the fields such as animal husbandry, industry, agricultural, its solid is white crystals or crystalline powder, soluble in water and alcohol, insoluble in ethers, toluene and carbon tetrachloride, aqueous solution, in acidity, starts time melted to decompose to give off carbon dioxide and ammonia.
Embodiment one
A kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer that the present embodiment provides, mainly comprises the steps that
1) adopting phosphoric acid is that 1.2:1 mixes with phosphoamide according to mol ratio, and is warming up to 160 DEG C for 6 DEG C/min from 80 DEG C with programming rate, stirring reaction 4-5h, and separation obtains intermediate；Adopting this intermediate again is that 1:1.4 mixes with alkaline potassium salt according to mol ratio, regulating pH value is 8.5, after reaction terminates, obtain slip nitrogenous, phosphorus, potassium, and the slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer and cools to 35～40 DEG C, carry out crystallization filtration treatment, make filtrate circulation crystallization in cooler crystallizer process, the filter cake obtained is dikalium phosphate product, the component content in detection filtrate；
2) in filtrate, formalin is added, according to being that 0.8:1 mixes with the mol ratio of the phosphoamide contained in solution, with calcium hydroxide, potassium hydroxide and phosphoric acid solution regulate the pH value of solution, wherein calcium hydroxide concentration is 40%, the concentration of potassium hydroxide is 20%, the concentration of phosphoric acid solution is 20%, when detecting that the pH value of solution is 9.0, the content of nitrogen component is 18-25%, phosphorus composition content is 4-8%, when potassium component content is 12-16%, when calcium component content is 12～18%, mixed liquor is put in retort, pressure is increased to 8～10 atmospheric pressure, be rapidly heated 85 DEG C time, ramp with 5～6 DEG C/min, when reaching 120 DEG C, keep 2～3h；
3) by step 2) solution that obtains is divided into two parts,
The solution fast cooling taking a deal to 60 DEG C and is depressurized under normal pressure and stands, called after solution A,
The solution taking a deal is put in a retort, when atmospheric pressure is quickly ramped up to 2 atmospheric pressure, increases atmospheric pressure with the speed of 50～100Pa/min, simultaneously temperature is from 85 DEG C of ramp with 1～2 DEG C/min, when reaching 3 atmospheric pressure, temperature is when reaching 95 DEG C, keeps 0.5～1h, called after solution B；
4) by step 3) solution A that obtains, it is cooled to 60～65 DEG C after B mixing, and add a certain amount of H2SO4Solution, regulates the scope of pH to 7.0, and described sulfuric acid concentration is 15%, is subsequently adding at least one in a small amount of zinc sulfate, copper sulfate, manganese sulfate, ammonium molybdate, ferrous sulfate, chelated iron, Borax, stands 0.5～1h, obtains solution C；
5) by step 4) in the solution C that obtains be cooled to 20～25 DEG C, carry out crystallization filtration treatment, obtain substantial amounts ofThe potassium phosphate of root, and a small amount ofWithDeng the chemical combination state compound fertilizer just finished product of urea aldehyde, when the content of the nitrogen component in chemical combination state compound fertilizer just finished product be 16%, phosphorus composition content be 7%, potassium component content be 11% time, calcium component content be 15% time, stop crystallization；
6) pelletize is dried, in this step, first by step 5) mixture that precipitates out is fabricated to the granule that diameter is 0.2～0.4cm, be subsequently placed in temperature be 45～50 DEG C, flow velocity be 3～4m/s ammonia environment in dry, making osmanthus fragrans special fertilizer, this special fertilizer is the Chemical Mixed Fertilizer of chemical combination state.
Embodiment two
A kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer that the present embodiment provides, mainly comprises the steps that
1) adopting phosphoric acid is that 1.5:1 mixes with phosphoamide according to mol ratio, and is warming up to 160 DEG C for 6 DEG C/min from 80 DEG C with programming rate, stirring reaction 4-5h, and separation obtains intermediate；Adopting this intermediate again is that 1:1.1 mixes with alkaline potassium salt according to mol ratio, regulating pH value is 8.5, after reaction terminates, obtain slip nitrogenous, phosphorus, potassium, and the slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer and cools to 35～40 DEG C, carry out crystallization filtration treatment, make filtrate circulation crystallization in cooler crystallizer process, the filter cake obtained is dikalium phosphate product, the component content in detection filtrate；
2) in filtrate, formalin is added, according to being that 0.9:1 mixes with the mol ratio of the phosphoamide contained in solution, with calcium hydroxide, potassium hydroxide and phosphoric acid solution regulate the pH value of solution, wherein calcium hydroxide concentration is 35%, the concentration of potassium hydroxide is 25%, the concentration of phosphoric acid solution is 25%, when detecting that the pH value of solution is 9.0, the content of nitrogen component is 18-25%, phosphorus composition content is 4-8%, when potassium component content is 12-16%, when calcium component content is 12～18%, mixed liquor is put in retort, pressure is increased to 8～10 atmospheric pressure, be rapidly heated 85 DEG C time, ramp with 5～6 DEG C/min, when reaching 120 DEG C, keep 2～3h；
3) by step 2) solution that obtains is divided into two parts,
The solution fast cooling taking a deal to 60 DEG C and is depressurized under normal pressure and stands, called after solution A,
The solution taking a deal is put in a retort, when atmospheric pressure is quickly ramped up to 2 atmospheric pressure, increases atmospheric pressure with the speed of 50～100Pa/min, simultaneously temperature is from 85 DEG C of ramp with 1～2 DEG C/min, when reaching 3 atmospheric pressure, temperature is when reaching 95 DEG C, keeps 0.5～1h, called after solution B；
4) by step 3) solution A that obtains, it is cooled to 60～65 DEG C after B mixing, and add a certain amount of H2SO4Solution, regulates the scope of pH to 7.4, and described sulfuric acid concentration is 5%, is subsequently adding at least one in a small amount of zinc sulfate, copper sulfate, manganese sulfate, ammonium molybdate, ferrous sulfate, chelated iron, Borax, stands 0.5～1h, obtains solution C；
5) by step 4) in the solution C that obtains be cooled to 20～25 DEG C, carry out crystallization filtration treatment, obtain substantial amounts ofThe potassium phosphate of root, and a small amount ofWithDeng the chemical combination state compound fertilizer just finished product of urea aldehyde, when the content of the nitrogen component in chemical combination state compound fertilizer just finished product be 19%, phosphorus composition content be 3%, potassium component content be 14% time, calcium component content be 10% time, stop crystallization；
6) pelletize is dried, in this step, first by step 5) mixture that precipitates out is fabricated to the granule that diameter is 0.2～0.4cm, be subsequently placed in temperature be 45～50 DEG C, flow velocity be 3～4m/s ammonia environment in dry, making osmanthus fragrans special fertilizer, this special fertilizer is the Chemical Mixed Fertilizer of chemical combination state.
Embodiment three
A kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer that the present embodiment provides, mainly comprises the steps that
1) adopting phosphoric acid is that 1.3:1 mixes with phosphoamide according to mol ratio, and is warming up to 160 DEG C for 6 DEG C/min from 80 DEG C with programming rate, stirring reaction 4-5h, and separation obtains intermediate；Adopting this intermediate and alkaline potassium salt again is 1:1.3 according to mol ratio, mixing, regulating pH value is 8.7, after reaction terminates, it is thus achieved that the slip of nitrogenous, phosphorus, potassium, and the slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer and cools to 35～40 DEG C, carry out crystallization filtration treatment, make filtrate in cooler crystallizer circulation crystallization process, it is thus achieved that filter cake be dikalium phosphate product, detection filtrate in component content；
2) in filtrate, formalin is added, according to being that 0.85:1 mixes with the mol ratio of the phosphoamide contained in solution, with calcium hydroxide, potassium hydroxide and phosphoric acid solution regulate the pH value of solution, wherein calcium hydroxide concentration is 37%, the concentration of potassium hydroxide is 22%, the concentration of phosphoric acid solution is 22%, when detecting that the pH value of solution is 8.8, the content of nitrogen component is 18-25%, phosphorus composition content is 4-8%, when potassium component content is 12-16%, when calcium component content is 12～18%, mixed liquor is put in retort, pressure is increased to 8～10 atmospheric pressure, be rapidly heated 85 DEG C time, ramp with 5～6 DEG C/min, when reaching 120 DEG C, keep 2～3h；
3) by step 2) solution that obtains is divided into two parts,
The solution fast cooling taking a deal to 60 DEG C and is depressurized under normal pressure and stands, called after solution A,
The solution taking a deal is put in a retort, when atmospheric pressure is quickly ramped up to 2 atmospheric pressure, increases atmospheric pressure with the speed of 50～100Pa/min, simultaneously temperature is from 85 DEG C of ramp with 1～2 DEG C/min, when reaching 3 atmospheric pressure, temperature is when reaching 95 DEG C, keeps 0.5～1h, called after solution B；
4) by step 3) solution A that obtains, it is cooled to 60～65 DEG C after B mixing, and add a certain amount of H2SO4Solution, regulates the scope of pH to 7.2, and described sulfuric acid concentration is 10%, is subsequently adding at least one in a small amount of zinc sulfate, copper sulfate, manganese sulfate, ammonium molybdate, ferrous sulfate, chelated iron, Borax, stands 0.5～1h, obtains solution C；
5) by step 4) in the solution C that obtains be cooled to 20～25 DEG C, carry out crystallization filtration treatment, obtain substantial amounts ofThe potassium phosphate of root, and a small amount ofWithDeng the chemical combination state compound fertilizer just finished product of urea aldehyde, when the content of the nitrogen component in chemical combination state compound fertilizer just finished product be 18%, phosphorus composition content be 5%, potassium component content be 13% time, calcium component content be 13% time, stop crystallization；
6) pelletize is dried, in this step, first by step 5) mixture that precipitates out is fabricated to the granule that diameter is 0.2～0.4cm, be subsequently placed in temperature be 45～50 DEG C, flow velocity be 3～4m/s ammonia environment in dry, making osmanthus fragrans special fertilizer, this special fertilizer is the Chemical Mixed Fertilizer of chemical combination state.
In order to prove the beneficial effect that the present invention reaches better, the present embodiment also provides for following experimental example, specific as follows:
Experimental example one
Fertile in fertilizer with common N, P, K, Ca mixing, wherein the content of nitrogen component be 16%, phosphorus composition content be 7%, potassium component content when being 11%, calcium component content be 15%, make culture fluid, osmanthus fragrans is carried out soilless culture, after cultivating 30 days, in detection culture fluid, the content of N, P, K, Ca composition, observes its growing way, called after A1 simultaneously.
Experimental example two
The osmanthus fragrans special fertilizer being successful with embodiment one to embodiment tripartite's method is as fertilizer, make culture fluid, osmanthus fragrans is carried out soilless culture, after cultivating 15 days, 30 days, 50 days, the content of N, P, K, Ca composition in detection culture fluid respectively, observe its growing way simultaneously, be respectively designated as A2, A3, A4.
The concentration of the culture fluid in above experimental example is suitable for, and for prior art, this experimental example seldom elaborates, and above experimental example is with 20 strain osmanthus fragrans for testing result such as table 1, table 2 and table 3:
Table 1: the content of N, P, K, Ca composition after cultivating 15 days
Table 2: the content of N, P, K, Ca composition after cultivating 30 days
Table 3: the content of N, P, K, Ca composition after cultivating 50 days
Can be seen that from table 1～3, with common compound fertilizer compared with the osmanthus fragrans special fertilizer that the present invention produces, when cultivating detection in the 15th day, its N, P, K, the absorbing state difference of Ca is little, but to when within the 30th day, detecting, N in the osmanthus fragrans special fertilizer solution that the present invention produces, P, K, the content of Ca is significantly lower than common special fertilizer, to when within the 50th day, detecting, the common N in compound fertilizer's culture fluid, P, K, Ca component residue has 60～80% not absorb, and the N in the culture fluid of the osmanthus fragrans special fertilizer that the present invention produces, P, K, Ca composition only remains 30～40% and is not absorbed, illustrate that the osmanthus fragrans special fertilizer that the present invention produces has the advantages that absorbance is good.
Meanwhile, this experimental example also observes the growing way situation that osmanthus fragrans was at the 15th day, the 30th day, the 50th day, is specially the above-mentioned experimental example of utilization and cultivates 50 strain osmanthus fragrans respectively, observes its growing way situation, such as table 4:
Table 4: osmanthus fragrans was the growing way situation of the 15th day, the 30th day, the 50th day
As can be seen from Table 4, in a short time, the fertile osmanthus fragrans special fertilizer produced with the present invention of common mixing is without much differences, when cultivating 30 days, there is malnutrition, leaf Huang phenomenon in the osmanthus fragrans that common mixed fertilizer is supported without earth culture, and the osmanthus fragrans that the osmanthus fragrans special fertilizer that the present invention produces is cultivated grows fine, its sprouting growing way is very fast, without yellow leaf phenomenon, during by the 50th day, stopping growing occurs in the osmanthus fragrans that common mixed fertilizer is supported without earth culture, and yellow leaf phenomenon is serious simultaneously, and the osmanthus fragrans growth that the osmanthus fragrans special fertilizer that the present invention produces is cultivated is relatively slowly, but without yellow leaf phenomenon.Illustrate that the osmanthus fragrans special fertilizer that the present invention produces has the effect of realizing controlled-release.
Claims (5)
1. prepare a production method for dikalium phosphate by-product osmanthus fragrans special fertilizer, mainly comprise the steps that
1) adopting phosphoric acid is (1.2-1.5) with phosphoamide according to mol ratio: 1 mixes, and is warming up to 160 DEG C for 6 DEG C/min from 80 DEG C with programming rate, stirring reaction 4-5h, and separation obtains intermediate；Adopting this intermediate again is 1:(1.1-1.4 with alkaline potassium salt according to mol ratio) mix, adjustment pH value is 8.5-9.0, after reaction terminates, obtain slip nitrogenous, phosphorus, potassium, and the slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer and cools to 35～40 DEG C, carry out crystallization filtration treatment, make filtrate circulation crystallization in cooler crystallizer process, the filter cake obtained is dikalium phosphate product, the component content in detection filtrate；
2) in filtrate, formalin is added, it is (0.8～0.9) according to the mol ratio with the phosphoamide contained in solution: 1 mixes, with calcium hydroxide, potassium hydroxide and phosphoric acid solution regulate the pH value of solution, when the pH value detected in solution is 8.5～9.0, the content of nitrogen component is 18-25%, phosphorus composition content is 4-8%, when potassium component content is 12-16%, when calcium component content is 12～18%, mixed liquor is put in retort, pressure is increased to 8～10 atmospheric pressure, be rapidly heated 85 DEG C time, ramp with 5～6 DEG C/min, when reaching 120 DEG C, keep 2～3h；
3) by step 2) solution that obtains is divided into two parts,
The solution fast cooling taking a deal to 60 DEG C and is depressurized under normal pressure and stands, called after solution A,
The solution taking a deal is put in a retort, when atmospheric pressure is quickly ramped up to 2 atmospheric pressure, increases atmospheric pressure with the speed of 50～100Pa/min, simultaneously temperature is from 85 DEG C of ramp with 1～2 DEG C/min, when reaching 3 atmospheric pressure, temperature is when reaching 95 DEG C, keeps 0.5～1h, called after solution B；
4) by step 3) solution A that obtains, it is cooled to 60～65 DEG C after B mixing, and add a certain amount of H2SO4Solution, regulates the scope of pH to 7.0～7.4, adds at least one in zinc sulfate, copper sulfate, manganese sulfate, ammonium molybdate, ferrous sulfate, chelated iron, Borax, stands 0.5～1h, obtains solution C；
5) by step 4) in the solution C that obtains be cooled to 20～25 DEG C, carry out crystallization filtration treatment, obtainThe potassium phosphate of root, andWithThe chemical combination state compound fertilizer just finished product of urea aldehyde；
6) pelletize is dried, in this step, first by step 5) mixture that precipitates out is fabricated to the granule that diameter is 0.2～0.4cm, be subsequently placed in temperature be 45～50 DEG C, flow velocity be 3～4m/s ammonia environment in dry, make osmanthus fragrans special fertilizer.
2. a kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer as claimed in claim 1, it is characterized in that: described calcium hydroxide concentration is 35～40%, the concentration of described potassium hydroxide solution is 20～25%, and the concentration of described phosphoric acid solution is 20～25%.
3. a kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer as claimed in claim 1, it is characterised in that: described step 4) sulfuric acid concentration be 5～15%.
4. a kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer as claimed in claim 1, it is characterized in that: when the content of the nitrogen component in chemical combination state compound fertilizer just finished product is 16-19%, phosphorus composition content be 3-7%, potassium component content be 11-14% time, calcium component content be 10-15% time, stop crystallization.
5. a kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer as claimed in claim 1, it is characterised in that: described osmanthus fragrans special fertilizer is the Chemical Mixed Fertilizer of chemical combination state.
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